EP1528049A1 - Procédé de fabrication d'un matériau composite en céramique - Google Patents

Procédé de fabrication d'un matériau composite en céramique Download PDF

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Publication number
EP1528049A1
EP1528049A1 EP04025471A EP04025471A EP1528049A1 EP 1528049 A1 EP1528049 A1 EP 1528049A1 EP 04025471 A EP04025471 A EP 04025471A EP 04025471 A EP04025471 A EP 04025471A EP 1528049 A1 EP1528049 A1 EP 1528049A1
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EP
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Prior art keywords
silicon
silicon carbide
production
pyrolysis
ceramic
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EP04025471A
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German (de)
English (en)
Inventor
Peter Prof. Dr. Greil
Heino Dr. Sieber
Lars Weisensel
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Viessmann Generations Group GmbH and Co KG
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Viessmann Werke GmbH and Co KG
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
    • C04B35/6267—Pyrolysis, carbonisation or auto-combustion reactions
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0022—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof obtained by a chemical conversion or reaction other than those relating to the setting or hardening of cement-like material or to the formation of a sol or a gel, e.g. by carbonising or pyrolysing preformed cellular materials based on polymers, organo-metallic or organo-silicon precursors
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/428—Silicon
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/46—Gases other than oxygen used as reactant, e.g. nitrogen used to make a nitride phase
    • C04B2235/465—Ammonia
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • C04B2235/483—Si-containing organic compounds, e.g. silicone resins, (poly)silanes, (poly)siloxanes or (poly)silazanes
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/80—Phases present in the sintered or melt-cast ceramic products other than the main phase

Definitions

  • the invention relates to a method for producing a Composite body of ceramic, in which a carbonaceous and cavities having shaped body formed, then subjected to pyrolysis and a siliconization and up to Training of silicon carbide is fired.
  • the invention relates Further, a silicon carbide-containing composite body.
  • SiC-based materials are used for a variety of different Applications, especially where high strength at high temperatures or high corrosion resistance be required.
  • SiC-based ceramics increasingly as high temperature resistant materials for catalyst carriers, as kiln furniture, insulation materials, as substrate materials or for gas heating in pore burners or for solar systems as well as for exhaust gas purification high temperatures required as filter materials.
  • biogenic raw materials are fiber composites in the form of nonwovens, mats or fabrics, ie Long fiber composites made of natural fibers, as well as large-area thin-walled Sheets proposed.
  • DE 101 61 108 A1 and WO 03/050058 A1 describe a method that using a fiber, span and / or strand Georgian cellulose-containing semi-finished homogeneous density distribution and Homogeneous structure produces a carbon or ceramic component.
  • semi-finished moldings are used in particular plate-shaped Moldings with homogeneous density distribution of celluloseund / or lignocellulose-containing particles prepared from Wood or vegetable fibers.
  • Homogeneous large-area carbon or ceramic components produced as mass products be that largely non-directional mechanical and have thermal properties.
  • DE 199 47 731 A1 (component made of SiC ceramic and method for Production of a component made of SiC ceramic) describes a Method for producing a component made of SiC ceramic under Use of a starting body made of cellulosic material and binder, characterized in that the Starting body consists of a technical semi-finished, the In the form of chips and / or one or more Layers of cellulosic material bonded with pyrolyzable material Binder is produced.
  • Ceramic material describes a ceramic Material and a method for its production in which a charred material coked and then with Si is infiltrated.
  • Wood and plants and woody products e.g. described.
  • the shaping can be described in the Process after pyrolysis or after silicization respectively.
  • EP 1 219 578 A2 (silicone / silicon carbide composite and process for manufacturing the same) describes a method of production of moldings of SiSiC ceramic with 45-75 wt .-% Si and 25-55 wt% SiC from an array of cellulosic fibers with a thickness of 150 mm and a length of 0.8 - 3.5 mm.
  • the process describes the preparation of particular dense, high purity SiSiC materials for semiconductor temperature treatment without going into the shape of the same.
  • EP 0 151 213 A1 describes a process for the production a reaction sintered silicon carbide body with porous Structure.
  • This is a still deformable, strong carbonaceous Pre-body brought into the desired final shape and by a per se known method with exclusion of air coked so that the carbon skeleton remains behind (pyrolysis).
  • the carbonized parts are associated with silicon (Silication).
  • silicon is deposited by decomposition and in another thermal process for reaction C + Si -> SiC brought.
  • the object of the invention is therefore a process for the preparation of silicon carbide composites to provide the cheaper and easier to perform.
  • the invention is based on the surprising finding that for the production of silicon carbide-containing composites is not required, a special precursor high-carbon raw materials, but that already commercially available corrugated board, despite their significantly lower carbon content are suitable, silicon carbide - Ceramics with sufficiently good for practice To produce properties.
  • corrugated board here is any commercial paper product understood, in which one or more sheets of paper or Cardboard joined together to form a voided body is.
  • the invention makes it possible to use in the paper industry developed various possibilities of paper processing and molding for the production of ceramics exploit. Especially can single-layered, as well as single and multi-wave Corrugated cardboard are used. Ceiling and wave papers of Corrugated board can be made from virgin fiber (wood pulp) as well be made from waste paper. Depending on the fiber composition a distinction is made between the corrugated base papers kraftliner and testliner or Schrenz as cover papers and half-pulp paper or corrugated medium as wave papers, each for different Purpose also in the ceramic production can be used.
  • An overview of commercially produced Corrugated cardboard, their manufacture and properties can be found in the DIN 55468 as well as on the Internet side of the federation of the German corrugated cardboard industry (http: ⁇ www.wellpappen-industrie.de).
  • An inventive, SiC-containing composite body is thus characterized by the following manufacturing steps: the manufacture of a preform made of corrugated cardboard this is under Anhydrous or a low-oxygen inert gas coked and subsequently with silicon or silicon-containing compounds brought into contact.
  • the silicon or the silicon-containing Compounds can be solid, liquid or gaseous Form are brought to the coked preform.
  • the in this way brought into contact with silicon preform be in a further or simultaneous step subjected to a heat treatment, which makes it to the implementation of C and Si come in SiC.
  • the heat treatment can also additional steps, such as frying or sintering, to the properties of the composite in the desired manner influence.
  • the implementation in ceramic SiC-based components is about a simple, 1- or 2-stage tempering treatment in inert Atmosphere possible.
  • the converted ceramic components have the advantages of ceramic materials, e.g. High temperature resistance, and can be used in aggressive environmental conditions be used. With the method can also porous components made of SiC-based ceramic with closed pore structures are produced.
  • the pyrolysis of corrugated cardboard which if necessary to increase the Carbon density with dilute or undiluted solutions from cokemable substances (e.g., resins, lignin, sugar solutions) infiltrated takes place at a temperature between about 600 - 1800 ° C in inert, oxygen-free atmosphere instead.
  • cokemable substances e.g., resins, lignin, sugar solutions
  • the cellulose fibers, or the cokokstoffen in To prevent carbon arising gases should be up to a temperature of about 400-500 ° C, a slow heating rate selected (eg 1-2 ° C / min). From about 500 ° C can be a higher Heating rate (eg 5 ° C / min) can be used.
  • the pyrolysis temperature should be kept for about 1h.
  • the silicization of the pyrolyzed components preferably in the form a melt phase silicidation found under oxygen free Atmosphere or in vacuo (about 100 Pa) instead.
  • Well suited a Wicksilizierung in which the pyrolyzed component on a porous carbon or SiC body is provided and the liquid Si flows into the component via the porous wick. Due to the porous structure of carbon is a spontaneous infiltration of the component with the liquid Si and a conversion of the carbon to SiC. After silicating at temperatures between about 1420 - 1600 ° C, the component relatively easy and without destroying it again separated from the wick become.
  • other types of silicidation are also suitable, z. B. in which the component directly into a powder bed is made of Si.
  • the silicization can be another treatment step follow, in which the silicon at least is partially removed, creating a ceramic with elevated SiC content is produced.
  • the two-stage process of pyrolysis and silicization may be summarized in a one-step process become.
  • the one-step litigation will also be characterized favors that unlike the pyrolysis of woody Starting materials in the use of paper products a much lower burden of decomposition products occurs during pyrolysis, since a much lower Amount of cellulosic starting materials in the ratio to the component size is available.
  • the corrugated fiberboards may also be subjected to infiltration with an Si-containing preceramic compound, such as TEOS tetraethyl orthofosilicate, polysiloxane, polycarbosilane or polysilazane, and / or Si / SiO 2 powder, followed by pyrolysis, wherein the reactive reaction is in SiC ceramic inert atmosphere at temperatures above about 600 ° C is performed.
  • an Si-containing preceramic compound such as TEOS tetraethyl orthofosilicate, polysiloxane, polycarbosilane or polysilazane, and / or Si / SiO 2 powder
  • the composite body After formation of silicon carbide, the composite body can also be coated by a tempering treatment in air at temperatures above about 600 ° C with a surface layer of SiO 2 .
  • the pictures show an example of some concrete applications for the invention described, but the invention is not limited thereon.
  • One picture is shown in the pictures Corrugated cardboard molded preform and the resulting - after processing according to the inventive method - resulting ceramic composites.
  • Example 1 Figure 1 - SiSiC component with uniaxially oriented cell structure
  • Single-sided corrugated board with different wave height and wave width are rolled up and glued to cylindrical components (picture 1, left).
  • the result is components made of corrugated cardboard with directed pore structures with cell diameters between 1 to 8 mm and cell wall thicknesses corresponding to the selected paper thickness (about 200 ⁇ m).
  • To increase the mechanical strength of the rolled corrugated cardboard can be fitted in a likewise made of cardboard ring.
  • the corrugated components were pyrolyzed at 800 ° C in N 2 atmosphere. In this case, a slow heating rate of 1 ° C / min was used up to a temperature of 500 ° C. At this temperature, the thermal decomposition of the cellulose fibers to carbon is largely complete.
  • the mixture was then heated at a heating rate of 5 ° C / min to 800 ° C. After pyrolysis, a weight loss of 78% by weight was determined and a shrinkage of about 20% in the axial and radial directions.
  • the resulting carbon shapes retain the inner and outer shape of the corrugated board member and were reacted by subsequent infiltration with liquid Si at a temperature of 1500 ° C (holding time 1h) in SiSiC ceramics. After siliconization, a porous SiSiC ceramic (porosity approx. 60%) was created, which reflects the original form of the rolled corrugated cardboard component (Fig. 1, right).
  • SiSiC ceramics with uniaxial directed porosity can e.g. as catalyst carrier structures, for the transport of hot gases, for the heating of gases in solar systems, as kiln furniture or as pore burner substrates be used.
  • One-sided corrugated board with different wave height and Shaft width were rolled up and become cylindrical components glued (picture 2, left). It creates components made of corrugated cardboard with directed pore structures with cell diameters between 1 to 8 mm and cell wall thicknesses according to the selected paper thickness (about 200 microns). To strengthen the mechanical strength The rolled corrugated cardboard components became one too made of cardboard boxes existing ring. Before the pyrolysis The corrugated cardboard components were made with a coke Polymer (furan resin, undiluted) for increasing the carbon density the cell walls infiltrated at room temperature. The polymer infiltration led to an increase in weight of the corrugated cardboard component of about 50% by weight. The pyrolysis was analogous to Example 1 performed.
  • Single-sided or double-sided corrugated board with different Wave height and wave width are cut square each glued to each other with 90 °, (picture 3, Left). It creates components made of corrugated cardboard with crosswise directed Pore structures with cell diameters between 1 to 8 mm and cell wall thicknesses according to the selected paper thickness (about 200 microns).
  • the pyrolysis and silicization became analog Example 1 performed. After silicization are highly porous SiSiC ceramics were created, which are the original form of the reflect crosswise bonded corrugated board (Fig. 3, right).
  • Such, easy to produce SiSiC or SiC (after additional Treatment for the removal of Si) ceramics with Crosswise uniaxially directed cell structures may e.g. as heat exchanger structures at high temperatures or as Kiln furniture can be used.
  • Two-sided corrugated board with different wave height and Wavelength are cut into flat components (Fig. 4, Left).
  • the result is components made of corrugated cardboard with directional Pore structures with cell diameters between 1 and 8 mm and Cell wall thicknesses according to the selected paper thickness (approx. 200 ⁇ m).
  • the pyrolysis and silicization was carried out analogously to Example 1. After the silicization are planar, lightweight SiSiC ceramics, which are the reflect the original shape of the corrugated cardboard structures (Picture 4, right).
  • Such easy-to-produce and lightweight SiSiC ceramics can e.g. as high temperature stable substrates for z.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Dispersion Chemistry (AREA)
  • Ceramic Products (AREA)
EP04025471A 2003-10-31 2004-10-27 Procédé de fabrication d'un matériau composite en céramique Withdrawn EP1528049A1 (fr)

Applications Claiming Priority (2)

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DE10351057 2003-10-31
DE10351057 2003-10-31

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011000967A1 (fr) * 2009-07-03 2011-01-06 Schunk Kohlenstofftechnik Gmbh Procédé de préparation d’un corps céramique, d’un catalyseur de gaz d’échappement, ainsi que support pour celui-ci
WO2011015571A1 (fr) * 2009-08-04 2011-02-10 Schunk Kohlenstofftechnik Gmbh Procédé de fabrication d'un échangeur thermique et échangeur thermique
CN107010973A (zh) * 2017-05-10 2017-08-04 济南大学 一种轻质复相多孔隔热耐火材料和莫来石质耐火材料及其制备方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1368169A (en) * 1972-11-20 1974-09-25 Nippon Oil Seal Ind Co Ltd Production of silicon carbide articles
US4617072A (en) * 1983-07-30 1986-10-14 Mtu Motoren-Und Turbinen-Union Muenchen Gmbh Method for producing a composite ceramic body
EP1284251A1 (fr) * 2001-08-17 2003-02-19 Eiji Tani Matériau structural poreux, leger et resistant à chaleur à base de carbure de silicium, et son procédé de fabrication

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1368169A (en) * 1972-11-20 1974-09-25 Nippon Oil Seal Ind Co Ltd Production of silicon carbide articles
US4617072A (en) * 1983-07-30 1986-10-14 Mtu Motoren-Und Turbinen-Union Muenchen Gmbh Method for producing a composite ceramic body
EP1284251A1 (fr) * 2001-08-17 2003-02-19 Eiji Tani Matériau structural poreux, leger et resistant à chaleur à base de carbure de silicium, et son procédé de fabrication

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011000967A1 (fr) * 2009-07-03 2011-01-06 Schunk Kohlenstofftechnik Gmbh Procédé de préparation d’un corps céramique, d’un catalyseur de gaz d’échappement, ainsi que support pour celui-ci
WO2011015571A1 (fr) * 2009-08-04 2011-02-10 Schunk Kohlenstofftechnik Gmbh Procédé de fabrication d'un échangeur thermique et échangeur thermique
CN107010973A (zh) * 2017-05-10 2017-08-04 济南大学 一种轻质复相多孔隔热耐火材料和莫来石质耐火材料及其制备方法

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